反应详情

温度

50 °C

A solution of 4-[3-(4-ethoxycarbonyl-2-fluoro-phenoxy)-propyl]-piperazine-1-carboxylic acid tert-butyl ester from Example E39.1 (1.7 g, 4.1 mmol) in dioxan (25 ml) was treated with 2N NaOH (3 ml) and the mixture stirred at 50° C. for 18 h. A further aliquot of 2N NaOH was added (2 ml), and stirring continued at 50° C. for 3 h. Solvents were removed in vacuo and azeotroped with toluene. The residue was purified by flash chromatography on silica gel (eluant; 1% acetic acid:9% methanol:90% chloroform) to yield the title compound (1.45 g, 92%).

1. stirringstirring
2. waitcontinued at 50° C. for 3 h
3. customSolvents were removed in vacuo
4. customazeotroped with toluene
5. customThe residue was purified by flash chromatography on silica gel (eluant; 1% acetic acid:9% methanol:90% chloroform)